CN103820072A - Double-component silicone structural sealant for heat mirror hollow glass and preparation method thereof - Google Patents
Double-component silicone structural sealant for heat mirror hollow glass and preparation method thereof Download PDFInfo
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- CN103820072A CN103820072A CN201210468036.3A CN201210468036A CN103820072A CN 103820072 A CN103820072 A CN 103820072A CN 201210468036 A CN201210468036 A CN 201210468036A CN 103820072 A CN103820072 A CN 103820072A
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Abstract
The invention discloses a double-component silicone structural sealant for heat mirror hollow glass and a preparation method of the sealant. The sealant comprises a component A and a component B, wherein the component A comprises hydroxyl-terminated polydimethylsiloxane, alkyl-terminated polydimethylsiloxane, hollow microsphere, ceramic microbead, metal hydroxide, metal oxide, activated calcium carbonate, inorganic pigment and a surfactant; the component B comprises alkyl-terminated polydimethylsiloxane, a coupling agent, a cross-linking agent, a catalyst, an inhibitor, a thickening agent, and silicon dioxide. The preparation method of the sealant comprises the following steps: 1) taking each ingredient in the component A to be mixed uniformly under the vacuum condition; 2) taking each ingredient in the component B to be mixed uniformly under the vacuum condition; 3) mixing the component A and the component B at room temperature according to the weight ratio of (8:1) to (20:1), and at last obtaining the sealant. The double-component silicone structural sealant is good in adhesiveness, high in curing speed, good in sealing performance, high in hardness and modulus, and excellent in thermal barrier effect, and suitable for sealing and bonding of heat mirror film, glass and metal materials etc.
Description
Technical field
The invention belongs to seal gum technical field, be specifically related to two component silicone structure sealants and preparation method thereof for a kind of heat mirror double glazing.
Background technology
Heat mirror double glazing can be rated as the glassy product of saving the most in the world at present the energy, is a kind of one deck to be shown to the polyester film of plated film is suspended on the two-chamber hollow or the multi-cavity hollow structure that between two or multi-disc glass, form.There is following characteristics compared with ordinary insulating glass: high-efficiency shielding ultraviolet ray, the ultraviolet ray of maskable 99.5%; Efficient sound insulation, than the barrier performance of at least many 5 decibel values of ordinary insulating glass; Energy-efficient, can effectively reduce summer air-conditioning and winter heating installation the huge electricity charge and energy expenditure; Not dewfall, the heat-insulating property of heat mirror excellence makes the temperature difference remain on double glazing both sides and has reduced heat loss and the accumulation of interior sheet double glazing, and the internal temperature of heat mirror double glazing and room temperature are approached, and avoids dewfall; Very low deadweight, at least reduces by 1/3 with common multiple glazing phase weight/power ratio, can greatly reduce transportation and laid down cost.
The seal gum performance requriements that heat mirror double glazing is used is higher than ordinary insulating glass.First to there is the splendid adhesive property of pair glass, metal and heat mirror films, also need higher hardness and higher modulus.The seal gum that heat mirror double glazing is conventional has polyurethane sealant and silicone sealant.Polyurethane sealant can not be heat-resisting for a long time, and light color formula is easily subject to ultraviolet aging, stability in storage packed and ectocine larger; poor water resistance, bad adhesion, many occasions need primary coat, and package encapsulation requires high; work-ing life is short, and large-scale production difficulty is large.Silicone sealant has remarkable ultraviolet resistance and atmospheric aging performance, under the comparatively severe condition such as sunlight, rain, snow and seasonal climate variation, use still can keep not chapping, the superior weather resistance of stay-in-grade, the advantage such as resist displacement deformability is strong.Because silicone sealant main chain is nonpolar-Si-O key, and heat mirror films is generally polyester film, its main chain is nonpolar-COO key, wettability between the two, interpenetrate power and bonding power a little less than, therefore, the bad adhesion of general silicone sealant and heat mirror films.In addition, on market, existing silicone structure sealant hardness is low, modulus is little, elasticity is large, is subject to ambient temperature to affect the shrinkage and expansion deformation of generation larger, easily causes heat mirror films distortion, increases the difficulty of heat mirror hollow glass production.At present, the limitations restrict of these two kinds of seal gums the large-area popularization and application of heat mirror double glazing.
In the prior art, as Chinese patent CN101831271A discloses a kind of double glazing bi-component organosilicone sealant, sealing glue has that low steam percent of pass, modulus are suitable, good weatherability, but because it uses conventional tackifier, unrestraint agent and tensio-active agent, common double glazing can only be used for, the requirement of heat mirror films for cohesive force and set time can not be met.And for example CN102352214A discloses a kind of pair of component silicone structure sealant, sealing glue has good ageing resistance and cohesiveness, but it uses conventional undressed filler, addition manner is single, without fire retardant, tensio-active agent, tackifier and inhibitor, can not meet double glazing heat mirror films to seal gum hardness, modulus, flame retardant resistance and thixotropic requirement.
Summary of the invention
The object of this invention is to provide two component silicone structure sealants for a kind of heat mirror double glazing, good to material bindings such as heat mirror films, glass and metals, curing speed fast, good airproof performance.
Second object of the present invention is to provide the preparation method of a kind of heat mirror double glazing with two component silicone structure sealants.
In order to realize above object, the technical solution adopted in the present invention is: two component silicone structure sealants for a kind of heat mirror double glazing, comprise A component and B component, and in described A component, each component and mass fraction are:
In described B component, each component and mass fraction are:
The mass ratio of A component and B component is 8:1～20:1.
The viscosity of described hydroxy-end capped polydimethylsiloxane is 1000cp～200000cp; The viscosity of described alkyl-blocked polydimethylsiloxane is 50cp～10000cp.
Before described cenosphere uses, through coupling agent treatment, particle diameter is nano level or micron order; Before described ceramic fine bead uses, through coupling agent treatment, particle diameter is nano level or micron order; Before described activated Calcium carbonate uses, through coupling agent or stearic acid processing, median size is 20～50nm; Described silicon-dioxide is any one or combination of aerosil, sedimentation silicon-dioxide, before using through coupling agent treatment.
Described metal hydroxides is any one or a few in aluminium hydroxide, magnesium hydroxide, zinc hydroxide; Described metal oxide is any one or a few in aluminum oxide, magnesium oxide, zinc oxide.
Described mineral dye is any one or a few in carbon black, red iron oxide, iron oxide yellow, titanium nickel yellow, titanium chromium palm fibre, cobalt blue, cobalt green, barba hispanica; Described tensio-active agent is any one or a few of Tegin 55G, sucrose ester, polysorbate.
Described coupling agent is any one or a few of γ-aminopropyl methyldiethoxysilane, N-(β-aminoethyl)-γ-aminopropyl methyl dimethoxysilane, γ-aminopropyl triethoxysilane, γ-(2,3-epoxy the third oxygen) propyl trimethoxy silicane; Described linking agent is any one or a few of methyltrimethoxy silane, dimethyldimethoxysil,ne, Union carbide A-162, poly-Union carbide A-162.
Described inhibitor is any one or a few in γ-mercaptopropyl trimethoxysilane, gamma-mercaptopropyltriethoxysilane, γ-glycidyl ether oxygen propyl trimethoxy silicane, γ-methacryloxypropyl trimethoxy silane.
Described catalyzer is any one in the ethyl acetoacetate chelate of dibutyltin diacetate, dibutyl tin laurate, Dibutyltin oxide, isopropyl titanate, tetrabutyl titanate, isopropyl titanate.
The silicone oligomer that described tackifier are is 2～10 containing the polymerization degree of acyloxy, epoxy group(ing) or alkoxyl group, preparation method is in the mixing solutions of silicon oil of low hydrogen content and Pt catalyzer, add any one in allyl acrylate, glycidyl allyl ether, vinyltrimethoxy silane, vinyltriethoxysilane, carry out addition reaction of silicon with hydrogen, temperature of reaction is 20～120 ℃, reaction times 4～10h, reaction finishes rear desolvation and get final product.
A preparation method for two component silicone structure sealants for heat mirror double glazing, comprises the following steps:
1) take respectively by weight hydroxy-end capped polydimethylsiloxane, alkyl-blocked polydimethylsiloxane, filler, fire retardant, mineral dye, tensio-active agent, be-0.090～-0.099MPa in vacuum tightness, rotating speed is to stir under the condition of 400～2000rpm, preparation A component;
2) take respectively by weight alkyl-blocked polydimethylsiloxane, coupling agent, linking agent, catalyzer, inhibitor, tackifier, silicon-dioxide, be-0.090～-0.099MPa in vacuum tightness, rotating speed is to stir under the condition of 400～2000rpm, preparation B component;
3) at room temperature A component and B component are mixed by weight 8:1～20:1, obtain described seal gum.
The present invention compared with prior art has the following advantages:
1) the present invention makes tackifier by oneself by interpolation, the cross-linking depth of silicone structure sealant is increased, and then improve its adhesive speed to heat mirror films, glass and metallic substance, and make tack time taper to above 1 day by original 7 days, improve greatly working efficiency.
2) cenosphere and ceramic fine bead are all that intensity is high, and the microballoon of hard hollow structure, it is higher than resistance, fusing point is high, do not decompose under high temperature, in seal gum, add these two kinds of materials not only can make it have larger hardness, higher modulus and good effect of heat insulation, but also can improve flame retardant resistance, the electrical insulating property of seal gum, meet the service requirements of heat mirror double glazing.
3) linking agent adopts organoalkoxysilane, not only can deepen the cross-linking depth of seal gum, improves hardness and its tensile bond strength.Linking agent is used in conjunction with inhibitor simultaneously, can also strengthen cohesive force, adjust set time, convenient construction.
4) in A component filler, add special metal oxide and metal hydroxides, can suppress flame, improve spontaneous ignition temperature, reduce flue dust, be enhanced to Jiaozhuo use, reduce thermal conduction rate, make the fire protection flame retarding rank of product reach difficult combustion rank B1 level, vertical combustion can reach FV-0 level.
5) add a certain amount of tensio-active agent, make seal gum obtain good thixotropy, convenient construction.
6) seal gum of the present invention can, according to engineering design demand modulates color, bring the enjoyment of people's visual aspects.
7) filler of selecting and mineral dye be nontoxic, environmental protection all.
Embodiment
Below in conjunction with embodiment, the present invention is further illustrated:
Embodiment 1
The heat mirror double glazing of the present embodiment comprises A component and B component with the two component silicone structure sealants of white, and in A component, each component and quality are:
In B component, each component and mass fraction are:
The mass ratio of A component and B component is 8:1.
The silicone oligomer that tackifier are is 2 containing the polymerization degree of acyloxy, preparation method is in the mixing solutions of silicon oil of low hydrogen content and Pt catalyzer, adds allyl acrylate to carry out addition reaction of silicon with hydrogen, and temperature of reaction is 60 ℃, reaction times 5h, reaction finishes rear desolvation and get final product.
The preparation method of this pair of component silicone structure sealant, comprises the following steps:
1) taking respectively by weight hydroxy-end capped polydimethylsiloxane, the viscosity that viscosity is 5000cp is the alkyl-blocked polydimethylsiloxane of 10000cp, cenosphere, ceramic fine bead, aluminium hydroxide, aluminum oxide, activated Calcium carbonate, sucrose ester, in vacuum tightness be-0.090MPa, rotating speed is to stir under the condition of 400rpm, preparation A component;
2) taking respectively by weight viscosity is the alkyl-blocked polydimethylsiloxane of 10000cp, γ-(2,3-epoxy the third oxygen) propyl trimethoxy silicane, γ-aminopropyl triethoxysilane, dimethyldimethoxysil,ne, dibutyltin diacetate, γ-mercaptopropyl trimethoxysilane, tackifier, silicon-dioxide, in vacuum tightness be-0.090MPa, rotating speed is to stir under the condition of 400rpm, preparation B component;
3) at room temperature A component and B component are mixed by weight 8:1, obtain described seal gum.
Embodiment 2
The heat mirror double glazing of the present embodiment comprises A component and B component with yellow two component silicone structure sealants, and in A component, each component and quality are:
In B component, each component and mass fraction are:
The mass ratio of A component and B component is 14:1.
The silicone oligomer that tackifier are is 4 containing the polymerization degree of epoxy group(ing), preparation method is in the mixing solutions of silicon oil of low hydrogen content and Pt catalyzer, adds glycidyl allyl ether to carry out addition reaction of silicon with hydrogen, and temperature of reaction is 20 ℃, reaction times 9h, reaction finishes rear desolvation and get final product.
The preparation method of this pair of component silicone structure sealant, comprises the following steps:
1) taking respectively by weight hydroxy-end capped polydimethylsiloxane, the viscosity that viscosity is 10000cp is the alkyl-blocked polydimethylsiloxane of 1000cp, cenosphere, ceramic fine bead, magnesium hydroxide, zinc oxide, activated Calcium carbonate, iron oxide yellow, Tegin 55G, sucrose ester, in vacuum tightness be-0.095MPa, rotating speed is to stir under the condition of 1000rpm, preparation A component;
2) take respectively by weight alkyl-blocked polydimethylsiloxane, γ-aminopropyl triethoxysilane, poly-Union carbide A-162, methyltrimethoxy silane, dibutyl tin laurate, gamma-mercaptopropyltriethoxysilane, tackifier, the silicon-dioxide that viscosity is 1000cp, in vacuum tightness be-0.095MPa, rotating speed is to stir under the condition of 1000rpm, preparation B component;
3) at room temperature A component and B component are mixed by weight 14:1, obtain described seal gum.
Embodiment 3
The heat mirror double glazing of the present embodiment comprises A component and B component with red two component silicone structure sealants, and in A component, each component and quality are:
In B component, each component and mass fraction are:
The mass ratio of A component and B component is 20:1.
The silicone oligomer that tackifier are is 6 containing the polymerization degree of alkoxyl group, preparation method is in the mixing solutions of silicon oil of low hydrogen content and Pt catalyzer, adds vinyltrimethoxy silane to carry out addition reaction of silicon with hydrogen, and temperature of reaction is 120 ℃, reaction times 7h, reaction finishes rear desolvation and get final product.
The preparation method of this pair of component silicone structure sealant, comprises the following steps:
1) taking respectively by weight hydroxy-end capped polydimethylsiloxane, the viscosity that viscosity is 150000cp is the alkyl-blocked polydimethylsiloxane of 50cp, cenosphere, ceramic fine bead, zinc hydroxide, magnesium oxide, activated Calcium carbonate, red iron oxide, polysorbate, in vacuum tightness be-0.099MPa, rotating speed is to stir under the condition of 2000rpm, preparation A component;
2) take respectively by weight alkyl-blocked polydimethylsiloxane, N-(β aminoethyl)-γ-aminopropyl methyl dimethoxysilane, Union carbide A-162, Dibutyltin oxide, γ-glycidyl ether oxygen propyl trimethoxy silicane, tackifier, the silicon-dioxide that viscosity is 50cp, in vacuum tightness be-0.099MPa, rotating speed is to stir under the condition of 2000rpm, preparation B component;
3) at room temperature A component and B component are mixed by weight 20:1, obtain described seal gum.
Embodiment 4
The heat mirror double glazing of the present embodiment comprises A component and B component with blue two component silicone structure sealants, and in A component, each component and quality are:
In B component, each component and mass fraction are:
The mass ratio of A component and B component is 12:1.
The silicone oligomer that tackifier are is 8 containing the polymerization degree of alkoxyl group, preparation method is in the mixing solutions of silicon oil of low hydrogen content and Pt catalyzer, adds vinyltriethoxysilane to carry out addition reaction of silicon with hydrogen, and temperature of reaction is 40 ℃, reaction times 10h, reaction finishes rear desolvation and get final product.
The preparation method of this pair of component silicone structure sealant, comprises the following steps:
1) taking respectively by weight hydroxy-end capped polydimethylsiloxane, the viscosity that viscosity is 200000cp is the alkyl-blocked polydimethylsiloxane of 2000cp, cenosphere, ceramic fine bead, magnesium hydroxide, aluminum oxide, activated Calcium carbonate, cobalt blue, polysorbate, in vacuum tightness be-0.093MPa, rotating speed is to stir under the condition of 1200rpm, preparation A component;
2) take respectively by weight alkyl-blocked polydimethylsiloxane, γ-aminopropyl methyldiethoxysilane, methyltrimethoxy silane, tetrabutyl titanate, γ-methacryloxypropyl trimethoxy silane, tackifier, the silicon-dioxide that viscosity is 2000cp, in vacuum tightness be-0.093MPa, rotating speed is to stir under the condition of 1200rpm, preparation B component;
3) at room temperature A component and B component are mixed by weight 12:1, obtain described seal gum.
Embodiment 5
The heat mirror double glazing of the present embodiment comprises A component and B component with green two component silicone structure sealants, and in A component, each component and quality are:
In B component, each component and mass fraction are:
The mass ratio of A component and B component is 10:1.
Tackifier are silicone oligomers that the polymerization degree of epoxy group(ing) is 10, preparation method is in the mixing solutions of silicon oil of low hydrogen content and Pt catalyzer, adds glycidyl allyl ether to carry out addition reaction of silicon with hydrogen, and temperature of reaction is 100 ℃, reaction times 4h, reaction finishes rear desolvation and get final product.
The preparation method of this pair of component silicone structure sealant, comprises the following steps:
1) taking respectively by weight hydroxy-end capped polydimethylsiloxane, the viscosity that viscosity is 80000cp is the alkyl-blocked polydimethylsiloxane of 5000cp, cenosphere, ceramic fine bead, zinc hydroxide, zinc oxide, activated Calcium carbonate, cobalt green, Tegin 55G, in vacuum tightness be-0.093MPa, rotating speed is to stir under the condition of 1200rpm, preparation A component;
2) take respectively by weight alkyl-blocked polydimethylsiloxane, γ-(2 that viscosity is 5000cp, 3-epoxy the third oxygen) propyl trimethoxy silicane, poly-Union carbide A-162, isopropyl titanate, γ-mercaptopropyl trimethoxysilane, gamma-mercaptopropyltriethoxysilane, tackifier, silicon-dioxide, in vacuum tightness be-0.093MPa, rotating speed is to stir under the condition of 1200rpm, preparation B component;
3) at room temperature A component and B component are mixed by weight 10:1, obtain described seal gum.
Embodiment 6
The heat mirror double glazing of the present embodiment comprises A component and B component with brown pair of component silicone structure sealant, and in A component, each component and quality are:
In B component, each component and mass fraction are:
The mass ratio of A component and B component is 17:1.
The silicone oligomer that tackifier are is 9 containing the polymerization degree of acyloxy, preparation method is in the mixing solutions of silicon oil of low hydrogen content and Pt catalyzer, adds allyl acrylate to carry out addition reaction of silicon with hydrogen, and temperature of reaction is 80 ℃, reaction times 6h, reaction finishes rear desolvation and get final product.
The preparation method of this pair of component silicone structure sealant, comprises the following steps:
1) taking respectively by weight hydroxy-end capped polydimethylsiloxane, the viscosity that viscosity is 1000cp is the alkyl-blocked polydimethylsiloxane of 500cp, cenosphere, ceramic fine bead, aluminium hydroxide, magnesium oxide, activated Calcium carbonate, titanium chromium palm fibre, sucrose ester, in vacuum tightness be-0.093MPa, rotating speed is to stir under the condition of 1200rpm, preparation A component;
2) take respectively by weight inner complex, γ-glycidyl ether oxygen propyl trimethoxy silicane, tackifier, the silicon-dioxide of the methyl aceto acetate of alkyl-blocked polydimethylsiloxane that viscosity is 500cp, N-(β-aminoethyl)-γ-aminopropyl methyl dimethoxysilane, methyltrimethoxy silane, isopropyl titanate, in vacuum tightness be-0.093MPa, rotating speed is to stir under the condition of 1200rpm, preparation B component;
3) at room temperature A component and B component are mixed by weight 17:1, obtain described seal gum.
Embodiment 1～6 gained seal gum the key technical indexes sees the following form 1:
Table 1 embodiment 1～6 gained seal gum the key technical indexes
Claims (10)
1. two component silicone structure sealants for heat mirror double glazing, is characterized in that: comprise A component and B component, in described A component, each component and mass fraction are:
The mass ratio of A component and B component is 8:1～20:1.
2. two component silicone structure sealants for heat mirror double glazing according to claim 1, is characterized in that: the viscosity of described hydroxy-end capped polydimethylsiloxane is 1000cp～200000cp; The viscosity of described alkyl-blocked polydimethylsiloxane is 50cp～10000cp.
3. two component silicone structure sealants for heat mirror double glazing according to claim 1, is characterized in that: before described cenosphere uses, through coupling agent treatment, particle diameter is nano level or micron order; Before described ceramic fine bead uses, through coupling agent treatment, particle diameter is nano level or micron order; Before described activated Calcium carbonate uses, through coupling agent or stearic acid processing, median size is 20～50nm; Described silicon-dioxide is any one or combination of aerosil, sedimentation silicon-dioxide, before using through coupling agent treatment.
4. two component silicone structure sealants for heat mirror double glazing according to claim 1, is characterized in that: described metal hydroxides is any one or a few in aluminium hydroxide, magnesium hydroxide, zinc hydroxide; Described metal oxide is any one or a few in aluminum oxide, magnesium oxide, zinc oxide.
5. two component silicone structure sealants for heat mirror double glazing according to claim 1, is characterized in that: described mineral dye is any one or a few in carbon black, red iron oxide, iron oxide yellow, titanium nickel yellow, titanium chromium palm fibre, cobalt blue, cobalt green, barba hispanica; Described tensio-active agent is any one or a few of Tegin 55G, sucrose ester, polysorbate.
6. according to two component silicone structure sealants for the heat mirror double glazing described in claim 1 or 3, it is characterized in that: described coupling agent is any one or a few of γ-aminopropyl methyldiethoxysilane, N-(β-aminoethyl)-γ-aminopropyl methyl dimethoxysilane, γ-aminopropyl triethoxysilane, γ-(2,3-epoxy the third oxygen) propyl trimethoxy silicane; Described linking agent is any one or a few of methyltrimethoxy silane, dimethyldimethoxysil,ne, Union carbide A-162, poly-Union carbide A-162.
7. two component silicone structure sealants for heat mirror double glazing according to claim 1, is characterized in that: described inhibitor is any one or a few in γ-mercaptopropyl trimethoxysilane, gamma-mercaptopropyltriethoxysilane, γ-glycidyl ether oxygen propyl trimethoxy silicane, γ-methacryloxypropyl trimethoxy silane.
8. two component silicone structure sealants for heat mirror double glazing according to claim 1, is characterized in that: described catalyzer is any one in the ethyl acetoacetate chelate of dibutyltin diacetate, dibutyl tin laurate, Dibutyltin oxide, isopropyl titanate, tetrabutyl titanate, isopropyl titanate.
9. two component silicone structure sealants for heat mirror double glazing according to claim 1, it is characterized in that: the silicone oligomer that described tackifier are is 2～10 containing the polymerization degree of acyloxy, epoxy group(ing) or alkoxyl group, preparation method is in the mixing solutions of silicon oil of low hydrogen content and Pt catalyzer, add any one in allyl acrylate, glycidyl allyl ether, vinyltrimethoxy silane, vinyltriethoxysilane, carry out addition reaction of silicon with hydrogen, temperature of reaction is 20～120 ℃, reaction times 4～10h, reaction finishes rear desolvation and get final product.
10. a preparation method for two component silicone structure sealants for heat mirror double glazing as claimed in claim 1, is characterized in that: comprise the following steps:
1) take respectively by weight hydroxy-end capped polydimethylsiloxane, alkyl-blocked polydimethylsiloxane, filler, fire retardant, mineral dye, tensio-active agent, be-0.090～-0.099MPa in vacuum tightness, rotating speed is to stir under the condition of 400～2000rpm, preparation A component;
2) take respectively by weight alkyl-blocked polydimethylsiloxane, coupling agent, linking agent, catalyzer, inhibitor, tackifier, silicon-dioxide, be-0.090～-0.099MPa in vacuum tightness, rotating speed is to stir under the condition of 400～2000rpm, preparation B component;
3) at room temperature A component and B component are mixed by weight 8:1～20:1, obtain described seal gum.
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